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    Assessment of external calibration, internal standard calibration and quadruple isotope dilution strategies for the determination of acrylamide in wastewater samples after LC-MS/MS quantification
    (Elsevier, 2023) Yazici, Elif; Bodur, Suleyman; Erarpat, Sezin; Arslan, Ulas Emre; Bakirdere, Sezgin
    Acrylamide is a possible neurotoxicant and carcinogen compound and its common usage in various industrial processes causes acrylamide contamination in environmental bodies. For this purpose, there is an increasing demand to develop an accurate and selective analytical method for the determination of acrylamide. In the scope of this study, external calibration (EC), internal standard calibration (ISC) and quadruple isotope dilution (ID4) strategies were compared to each other in terms of accuracy and precision. After the evaluation of these methods, liquid chromatography - quadruple isotope dilution - tandem mass spectrometry (LC-ID4-MS/MS) as a highly accurate and precise analytical approach was proposed to quantify acrylamide in wastewater samples. Several parameters for LC system such as sample injection volume, mobile phase type/composition and mobile phase flow rate were elaborately optimized to enhance peak shape and signal to noise ratio (S/N) belonging to the analyte. Under the optimum chromatographic and mass determination conditions, system analytical perfor-mance study was performed to determine dynamic range and limit of detection/quantitation (LOD and LOQ). LOD and LOQ values of the proposed LC-MS/MS method for the analyte were calculated as 1.18 and 3.93 mu g/kg; respectively. After the system analytical performance study, the spiking experiments in wastewater samples were carried out for the evaluation of accuracy and applicability of LC-MS/MS method. For wastewater samples, percent recovery results with their percent relative standard deviations (%RSD) obtained from EC, ISC and ID4 strategies were 115.8-177.8% (+/- 1.2-11.4%), 94.5-117.7% (0.3-4.7%) and 99.6-100.9% (0.4-1.7%); respec-tively. These results prove the superiority of ID4 strategy with regards to accuracy and precision of the results.
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    Cadmium determination at trace levels in lake water samples by cold vapor generation-atomic absorption spectrometry after magnetic dispersive solid phase extraction
    (Springer Int Publ Ag, 2023) Bodur, Suleyman; Erarpat, Sezin; Kayin, Inci; Bakirdere, Sezgin
    This study established an analytical method based on manganese ferrite based magnetic dispersive solid phase extraction (MDSPE) before cold vapor generation-atomic absorption spectrometry (CVG-AAS) for the determination of cadmium at trace levels in lake water samples collected from Horseshoe Island, Antarctica. Manganese ferrite nanoparticles were synthesized to be used as an adsorbent in the MDSPE method. Different MDSPE and CVG parameters were fixed to their optimum values after univariate optimization approach. Under the optimum conditions, analytical performance of the developed MDSPE-CVG-AAS method was evaluated and its applicability/accuracy was determined by recovery experiments. Twelve different lake water samples collected from Horseshoe Island, Antarctica were analyzed. Matrix matching calibration strategy was used to eliminate possible matrix effects arising from the lake water samples. Good recovery results (93.2-112.5%) were obtained from the spiked samples that indicated the method suitability to real samples.
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    Combination of high performance liquid chromatography and flame atomic absorption spectrophotometry using a novel nebulizer interface supported T shaped slotted quartz tube for the determination of Vitamin B12
    (Elsevier Science, 2022) Erarpat, Sezin; Bodur, Süleyman; Günkara, Ömer Tahir; Bakırdere, Sezgin
    A novel nebulizer interface (NI) was proposed to combine high performance liquid chromatography (HPLC) and flame atomic absorption spectrophotometer (FAAS). A glass concentric nebulizer was linked to T-shaped slotted quartz tube (T-SQT) using a tubing to transfer the liquid solution eluted from the chromatographic system into the atomization region of FAAS system. T-SQT was also used to intensify the interaction of atoms with the hollow cathode lamp light. Vitamin B12 was selected as an analyte to show the applicability of the new hyphenated system. After optimizing some parameters such as mobile phase flow rate and pH, nebulizer gas flow rate, T-SQT height and injection volume, linear range for the analyte was determined between 4.7 and 92 mg/kg as Co. Limit of detection (LOD) and limit of quantitation (LOQ) for the HPLC-NI-T-SQT-FAAS system were calculated to be 1.6 and 5.3 mg/kg as Co, respectively. Recovery studies were also conducted to verify the accuracy and applicability of the developed method for vitamin tablets and excellent percent recovery results (~ 100%) with low standard deviation values were obtained when matrix-matching calibration strategy was performed for each vitamin tablet. A successful separation and detection of the analyte was achieved within 3.0 min that offers high sample throughput. Two different vitamin tablets were analyzed by the optimized hyphenated system. The developed method also provides low usage of sample solution in contrast to conventional nebulizer in the FAAS system
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    A powerful combination of liquid chromatography-triple quadrupole mass spectrometry and quadruple isotope dilution strategy for the determination of fenuron at trace levels in river water, stream water and fruit juice samples
    (Academic Press Inc Elsevier Science, 2023) Bodur, Sueleyman; Erarpat, Sezin; Gunkara, Omer Tahir; Bakirdere, Sezgin
    An accurate, sensitive, and rapid analysis methodology for the determination of fenuron at ultratrace levels in river water, stream water and fruit juice samples was developed based on quadruple isotope dilution (ID4) and liquid chromatography-triple quadrupole mass spectrometry (LC-MS/MS) system. Fenuron-d6 as isotopically labelled material (ILM) was synthesized in our laboratory to apply the ID4 method. Optimization studies were performed to find experimental conditions for the separation and detection of fenuron at trace levels. Analytical performance parameters such as limit of detection (LOD), limit of quantitation (LOQ) and linear range were determined by external calibration strategy. LOD and LOQ values for the analyte were found at ppt levels and a wide linear range was obtained in the range of 0.11 - 492.4 & mu;g/kg. Recovery studies were also carried out for water and fruit juice samples to test applicability and accuracy of the developed LC-MS/MS system. ID4 strategy was applied to the selected samples to increase accuracy of the developed method and tolerate high matrix effects for fruit juice samples. According to high percent recoveries and low relative standard deviation values, the developed LC-ID4-MS/MS system was proven as an accurate, precise and sensitive analytical method for the quantification of fenuron at trace levels.
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    A simple spray assisted extraction/preconcentration of cadmium from sunflower oil, olive oil and hazelnut oil samples prior to flame atomic absorption spectrometry determination
    (Academic Press Inc., 2023) Erarpat, Sezin; Bakırdere, Sezgin; Bodur, Süleyman; Tutar, Ömer Faruk
    In this study, an efficient and simple analytical approach for the preconcentration and extraction of cadmium from sunflower oil, olive oil and hazelnut oil samples using environmentally friendly, easy and efficient vortex assisted reverse phase spray-based fine droplet formation liquid phase microextraction (VA-RP-SFDF-LPME) prior to flame atomic absorption spectrometry (FAAS) measurement was proposed. Limit of detection (LOD)/limit of quantification (LOQ) values were calculated as 2.89/9.62 µg/kg, 2.00/6.68 µg/kg and 4.77/15.92 µg/kg for sunflower oil, olive oil and hazelnut oil, respectively. Recovery experiments were carried out for the evaluation of applicability and accuracy of the developed method. Satisfactory recovery results for hazelnut oil, olive oil and sunflower oil samples were recorded in the range of 92.8 – 111.9%, 96.6 – 108.2% and 90.0 – 105.7%, respectively. These results verified that the proposed method can be accurately applied to the hazelnut oil, olive oil and sunflower oil samples to qualify/quantify their cadmium content. © 2023 Elsevier Inc.
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    Spray assisted preconcentration method combined with HPLC-Continuous flow hydride generation-FAAS for inorganic arsenic speciation in olive oil samples
    (Academic Press Inc Elsevier Science, 2023) Bodur, Sueleyman; Erarpat, Sezin; Tutar, Omer Faruk; Bakirdere, Sezgin
    Speciation analysis of arsenic in edible oils is an important topic in terms of the assessment of its risks for human health and the quality of edible oils. In this study, high performance liquid chromatography - continuous flow hydride generation - flame atomic absorption spectrometry (HPLC-CFHG-FAAS) system after vortex assisted reverse phase spray-based fine droplet formation liquid phase microextraction (VA-RP-SFDF-LPME) method was proposed to qualify/quantify arsenite and total arsenic. Limit of detection (LOD) and limit of quantification (LOQ) for arsenite were calculated as 2.86 & mu;g kg-1 (as As) and 9.52 & mu;g kg-1 (as As), respectively. After the extraction/preconcentration process, a prereduction was carried out in the presence of 0.010 mol/L HCl (con-taining 0.39% L-cysteine) with heat (90 & PLUSMN; 5 oC) for the determination of total arsenic content while arsenite was directly determined via the developed system. Recovery for arsenite and total inorganic arsenic were in the range of 91.5 - 120.4% and 90.0 - 104.4%, respectively. The developed method is proposed for the analysis of olive oil samples containing inorganic arsenic species. This is the first study to carry out the inorganic arsenic speciation in olive oil by HPLC-CFHG-FAAS system after the preconcentration of the species by the VA-RP-SFDF-LPME system. For the matrix including arsenite and arsenate, the developed method can be safely used to find the concentration of both species accurately.
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    Synthesis of Isotopic Labelled Paracetamol Benzoate-d3 and Its Application in the Determination of Paracetamol
    (Wiley-V C H Verlag Gmbh, 2023) Demirel, Rabia; Erarpat, Sezin; Bodur, Suleyman; Gunkara, Omer Tahir; Bakirdere, Sezgin; Turak, Fatma
    This study proposed a precise/accurate analytical method for the paracetamol (PCT) determination in human serum/urine matrices. PCT was simultaneously derivatized and preconcentrated by dispersive liquid-liquid microextraction (DLLME). Benzoyl chloride dissolved in dichloromethane was used as derivatization agent in the extraction solvent. Quadruple isotope dilution (QID) method with three calibration mixtures (A*B-x, x=1,2,3) and one sample mixture (AB) was performed to enhance the method accuracy and precision. In our research laboratory, paracetamol benzoate-d3 (PCT benzoate-d3) was synthesized and used as isotopically labelled substance (B) to conduct QID method. After the combination of QID and DLLME-GC-MS systems, percent recovery results for human serum/urine matrices were found to be 99.3-101.0 % and 98.8-99.9 %, respectively.